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1. Healthy and active Local Section organizations are vital factors in promoting the vigor and growth of the Institute. 2. Activity on the part of Local. Sections should be recognized and stim¬ulated by appropriation of funds from the Institute's treasury; and these appropriations should be as large as is consistent with the relative needs for other activities. 3. As between different Sections, the amount of such appropriations should be based primarily on the extent of activities as reflected in the number and character, of meetings held and the attendance of the members at such meetings. 4. In making a request for funds for any year, the officers of a Local Section should submit a report on the printed form approved by the Directors at their meeting on November 19, 1937. 5. A . standing Committee on Local Section Appropriations, consisting of one past chairman of a Local Section, one member of the Institute's Executive Committee, and one member of the Finance Committee, shall be appointed by the President and shall pass upon requests for appropriations and authorize payments within bounds of the budget. The committee will be guided by the principles herein outlined, always having in mind the vital importance of healthy, active sections to the welfare of the Institute as a whole.

Jan 1, 1938

CHICAGO SECTION CHARLES H. MACDOWELL, Chairman, Luther V. DICE, Vice-Chairman, HENRY WT. NICHOLS,. Secretary-Treasurer, 164.5 E. 68 St., Chicago; Ill. ALEXANDER K. HAMILTON-, HENRY P. HOWLAND, GEORGE P. HULST, FREDERICK 1. SNYDER. There were 32 members present at the dinner of the Chicago Section which was held at the Chicago Engineers' Club on Friday Evening, December 22. At the meeting after the dinner, the Chairman called attention to the work of Mr. Hoover in Belgium and spoke briefly of the assistance which' could be given him through the Belgian Kiddies, Ltd. Mr. Alonzo Kinyon read a paper on "Burring Powdered Coal" which so interested the members that many of them participated in the long discussion which followed. Prof. Harry B. Pulsifier then described the metallurgical plants about Chicago. He mentioned briefly the equipment and interesting features of 30 metallurgical plants of importance and stated that there were also 200 foundries in the district. He said that when number, size, quality and diversity of the plants are considered, the Chicago District is justified in calling itself the greatest metallurgical center on earth. The paper was followed by a brief discussion in Which attention was called to some smaller and incipient plants of an interesting character. HENRY T. NICHOLS, Secretary.

Jan 2, 1917

By A. T. Tye

WHEN the roughing tables operated in 1923 were abandoned, all the coarse iron pyrite for-merly removed by the tables had to be ground to flotation size, which caused an increased power con-sumption of 2 kw.-hr. per ton. Recently, by increasing the tonnage, this has been reduced to a total of 16.6 kw.-hr. per ton. The cost of repairs has been slightly reduced by using an alkaline circuit instead of the acid mine water used in 1923. Other economies from elim-inating roughing tables and the finishing tables have more than compensated for the extra grinding and the total costs have remained practically the same, until the first part of 1927, when, with increased tonnage, the total cost has decreased to 72 cents and the repair cost to 9 cents. In 1923, with a combined gravity and bulk flotation flowsheet, the grade of concentrate was only 4.38 per cent copper. With preferential flotation this has in-creased to over 17 per cent copper. The tailing has decreased from 0.29 per cent -copper to 0.18 per cent. The copper recovery, instead of decreasing; as might be expected, has increased from 87.4 per cent to, 91.5 per cent. The silver recovery has also increased from 88

Jan 8, 1927

By John Goheen

CONSIDERABLE work has been done in developing a pyrometer to measure the temperature of molten brasses, bronzes, and aluminum in the crucible. On account of the high melting points and the amount of zinc and sulfurous fumes given off from molten brasses, the conditions are somewhat severe for a thermocouple of standard design; but satisfactory results are obtained with a portable pyrometer, 3 ft. (0.9 m.) of connecting lead wire, and a special 5-ft. nickel-nickel chromium thermocouple, composed of rods ¼ in. (6.35 mm.) in diameter. The lower 12 or 24 in., as desired, may be made detachable so that new tips may be connected at little trouble or expense. The portable instrument need not be of the extreme high-resistance type, as the movable parts of the galvanometer of a lower resistance instrument may be better constructed to withstand the continuous handling such an instrument receives. Platinum-platinum rhodium thermocouples, protected with porcelain and graphite tubes, have been used, but the lag in registering the temperature is too great. It has been found that the range of temperature for various brasses is as follows: Red brasses 2200-2250° F. (1205-1234° C.) Yellow brasses 2250-2400° F. (1234-1318° C.) Bronzes 2300-2550° F. (1260-1400° C.)

Jan 11, 1921

By E. T. Dumble

THE development in the Gulf Coastal Plain for the year 1923 was entirely devoid of any spectacular feature and was considerably less than that of 1922. No large fields were discovered and the principal advances lay in the extension of the old fields and the finding of a new dome and other possible producing structures, which, however, so far, have given only small wells. While the production of some fields, such as those at Hull and Orange, was materially increased at times by comparatively large wells, the output as a whole shows a marked decrease over that of the preceding year. TABLE 1.-Production by Fields in Gulf Coastal Plain in 1923 FIELD BARRELS FIELD BARRELS Anse La Butte 16,942 Jennings 212,376 Barber's Bill 172,660 Markham 39,290 Batson 391,857 North D ayton 74,983 Big Hill (Jefferson County) 13,853 Orange 5,311,995 Blue Ridge 332,445 Pierce Junction 332,565 Damon Mound 822,355 Richmond (Big Creek) 17,545 Edgerley 176,964 Saratoga 700,661 Goose Creek 6,251,761 Sour Lake 2,091,961 High Island 19,018 Spindletop 309,315 Hull 7,732,139 Vinton 2,134,430 Humble 2,449,744 West Columbia 6,598,589 36,203,448

Jan 3, 1924

By J. Morgan Clements

PETROLEUM has been known in Japan since at least 668 A. D., for a picture shows the presentation, during that year, to the Emperor Tenchi (Tenji) of "burning water" and." burning earth" by his subjects from Echigo Province, which today is the largest producer of petroleum in Japan. The burning water was doubtless petroleum and the burning earth either bituminous shale or oil-soaked earth or rock from near the oil seepages. The early methods of getting the oil were simple and similar to methods used today in Japan and in China. Where the seepages occurred, trenches or shallow wells were dug along the seepages and allowed to fill with oil which was then bailed out; in some cases, they filled with oil and water and overflowed. During the 300 years following 1500 A. D:, the use of petroleum in Echigo Province seems to have increased considerably, as compared with earlier centuries, and records show that in 1818 the depth of the wells had been greatly increased. Doubtless, they passed through the seepages and tapped the shallow oil-bearing strata; probably some of these deeper wells were dug before that time. The real value of petroleum was not recognized until early in the Meiji era, which began in 1868, when the Japanese learned that the kerosene that was being imported was derived from petroleum. Guided solely by information obtained from books, they refined the oil and increased the depth of their wells in order to increase the production. The deepest well, dug by hand, about this time was 894 ft.1 (273 m.) and by 1874 the recorded production reached 3499 barrels. In 1876, Benjamin Smith Lyman prepared geological maps of the Echigo oil field, which were the first. of such geological maps made in Japan, and based on these a more enlightened development of the oil fields began; the. Japanese, however, still dug the wells by hand. Toward the end of the '80s, an American well-drilling outfit was secured, but the efforts to use it failed from lack of experience by the operators. In 1888, a complete well-drilling outfit was, purchased and American oil-well

Jan 7, 1922

Members whose deaths were reported from Apr. 5, 1920, to Apr. 9, 1921. Elected Died 1916 ALLAN, FERGUS L 1920 1916 ATKINSON, CHESTER 1921 1920 BARBERENA, RAUL R 1920 1918 BARKER, F. L 1920 1914 BELL, D. A. S 1920 1920 BREWSTER, GEORGE AUGUSTUS 1920 1917 BRIGHAM, EDMUND D 1921 1915 CARROLL, D. J 1920 1897 CHAPMAN, ROBERT H 1920 1919 COOPER, W. G 1920 1918 CRITCHLOW, EDWARD B 1920 1917 CURTIS, WILLIAM L 1920 1893 DARSIE, JAMES 1920 1892 DELANO, WARREN 1920 1877 DEWEY, FREDERIC P 1921 1917 ENEBO, BENJAMIN A 1920 1896 FAWCETT, JAMES H 1920 1906 FRASER, A LEXANDER J . 1920 1889 GARLICHS, HERMAN 1921 1893 GILLET, LORENZO M 1920 1886 HALDEMAN, HORACE L 1920 1914 HALL, HARRY E 1919 1905 CHART, C. R 1920 1906 HART, PHILIP E 1920 1877 HARTRANFT, SAMUEL S 1921 1914 HICKMAN, E C 1920 1919 || INMAN, WILLIAM ELLIOTT 1921 1920 JETER, J. TINSLEY 1920 1918 JOHNSON, CHARLES W 1920 1916 JOHNSON, FRANK E 1920 1913 KING, FREDERICK G 1921 1887 KNAPP, GEORGE F 1920 1902 LAMB, RICHARD 1920 1880 LANE, J. S 1920 1920 LECKIE, WILLIAM 1920 1887 LEVAT, DAVID 1921 1882 LAWRENCE, BENJAMIN B 1918 1916 LEYNER, J GEORGE 1920 1871 LYMAN, BENJAMIN S 1920 1903 MCCHRYSTAL, JOHN H1920

Jan 1, 1923

By J. G. Paterson, J. A. Meech

Abstract-Activated carbon is a strong adsorbent for amyl xanthate, capable of removing from solution up to a quarter of its own weight in xanthate. In selective flotation systems where depression is unstable, separation efficiency increases with activated carbon additions. The improvements observed are brought about by two mechanisms. First, by removing stripped and residual collector ions from solution, competition between depressant and xanthate is reduced and depression is stabilized. In addition, the texture of the froth phase at high pine oil concentrations is modified by activated carbon such that better drainage between the air bubbles takes place, alleviating the mechanical entrapment of depressed mineral particles. In treating a bulk copper/lead concentrate produced from GECO ore, selectively between galena and chalcopyrite is increased when activated carbon is used. Although the rate of flotation of galena is marginally lowered by activated carbon, a small extension in the duration of flotation allows the lead recovery to increase by 19% at the same recovery of copper. An addition rate of 0.75 kg/ton (1.5 lb/st) of bulk concentrate is suggested as optimum from this testwork. However, the actual level wed in the mill is dependent upon the residual concentrations of collector and frother in the bulk concentrate Pulp.

Jan 11, 1978

By John V. Beall

W hen the blasts went off on West 11th St., just off 5th Ave. in New York City, James Michaels, editor of Forbes magazine, was in his office a few doors away reviewing color layouts with his production manager. Having once been a reporter, he grabbed his trench coat and dashed for the street to be con- fronted by the demolished townhouse which had been turned into a bomb factory by youths. To Michaels, this shocking episode supplied the exclamation point to thoughts he was formulating that an era had ended and a new one was beginning in the economic and social climate of the U. S. "For twenty years corporate profits, the stock market, middle income pay have gone up and up. . . The illusions of twenty years are in confrontation today with changed needs," he said. "International omnipotence is economically beyond our means, . . The anti-pollution and community renewal people are not nuts in tennis shoes who will go away. . . That corporation presidents can report an increase in earnings every year is an illusion that will be dropped. . . There has been a $200 billion shrink in value of stocks and bonds since Nixon came into office" were some indicators Michaels mentioned.

Jan 1, 1970

Rustenburg Platinum Mines, Ltd. is the largest producer of platinum metals in the western world. It is also the only major platinum producer this side of the Iron Curtain. One of its mines is situated at Rustenburg, 80 miles northwest of Johannesburg. It also has a smaller operation, the Union Section, 60 miles north of the Rustenburg property. Both mines exploit the Merensky Reef, which forms a part of the Transvaal's remarkable Bushveld Igneous Complex, an irregular oval area covering some 15,000 square miles. In order to cope with an increasing world demand for platinum and such platinum-group metals as palladium, rhodium, ruthenium, iridium and osmium, Rustenburg Platinum Mines embarked on a major expansion program some time ago. It is expected that production will reach an annual rate of 850,000 oz of platinum by the middle of 1969 and increase to 1 million oz by the middle of 1970. Capital expenditures at Rustenburg during the next few years will be about $60 million. It is believed that the ore at Rustenburg averages about 4.5 oz of precious metals per ton. About 70% of the metal is platinum, some 15% is palladium, and the rest is made up of the other metals in the platinum group.

Jan 4, 1969

By M. C. Fuerstenau

Each year during the AIME Annual Meeting, the MBD Division has its Business Meeting. Because many members cannot attend, it has be- come policy for the secretary of the Division to present highlights of the business conducted at the Meeting in Fine Grind. This year the Meeting was held on March 1 in the Americana Hotel. Five major items of business were brought up for discussion. These were: (1) the proposed name change for the Division, (2) institution of the Taggart Award, (3) a name change for a Unit Committee, (4) MBD funding of scholarships, and (5) authorship of Fine Grind articles. The Matter of What We Should Call Ourselves A lively discussion was held on the issue of a name change for the Division. Two names have been proposed: (1) Mineral Processing Division, and (2) Mineral Engineering Division. A number of strong reasons for changing the name from Minerals Beneficiation Division have been pointed out. Perhaps the most important of these is that the term "beneficiation" does not describe all of the functions that engineers in our Division perform. Further, there are inherent problems associated in the term, in that beneficiation is a long word which has the twofold disadvantage of being both difficult to pronounce and difficult to spell.

Jan 1, 1971

By George L. Atwood, William Brown

Phosphate ore is being mined at Monsanto Co.'s Henry mine, near Soda Springs, Idaho, for the company's three furnace elemental phosphorus plant near Soda Springs. The finished product from the furnaces is elemental phosphorus which is subsequently used in the manufacture of detergents, food preservatives, fire retardants and other consumer items. In stripping and mining, D-9 crawler tractors are utilized to rip and push-load rubber-tired scrapers. The equipment consists of six D-9G crawler tractors, four Caterpillar 657B scrapers, eight Euclid S-24 scrapers, one Reich T750 drill and one Caterpillar No. 16 patrol plus various support equipment. Stripping is performed on a 12- month basis, two shifts per day, whereas mining is mainly in the summer months on a one-shift basis. The hauling season begins May 15 and ends November 1 due to freezing weather and snow conditions. Annual production is 1 million tons of phosphate rock and 2.5-3 million cu yd of stripping. Stripping, mining and hauling is performed for Monsanto by Dravo-Soda Springs, a mining contractor which owns, operates and maintains all equipment used. The contractor is paid for stripping by the bank yard and for ore mined and hauled on a tonnage basis.

Jan 8, 1972

APPLICATIONS for loan contracts for the exploration, development and mining of strategic and critical metals and minerals are now being accepted by the Department of the Interior. The RFC is authorized and directed by Executive Order 10161 to make such loans but the Secretary of the Interior must pass on the necessity for the loan. Applications should be addressed to James Boyd, acting deputy administrator, Defense Minerals Administration, Department of the Interior, Washington, D.C. rather than to the Field Offices of the Bureau of Mines as was first planned. Application forms are not yet available but it has been learned that data accompanying the application should include the known quantity and grade of reserves, the anticipated rate of production, the equipment, supplies, and man power required for the additional production, etc.

Jan 12, 1950

By Edmund J. Korber, Donald E. Raab, Frank A. Burns

During the early 1960s, the advent of self- advancing longwall roof supports triggered serious consideration by Bethlehem management to introduce the technique of longwall mining at one of our central Pennsylvania coal mines. Although longwall mining was initially justified as a means to cope with the severe roof conditions at our Mine 32 (Watson, B., 1971), the result of the endeavor has been a consistent and reliable level of coal production, first from Mine 32 and then later from Mine 33, over a period of fifteen years. Longwall production from the Cambria Division has been the mainstay of the low volatile coal required by Bethlehem Steel for steel production. Let us review the events that led to this accomplishment, as well as where we stand today.

Jan 1, 1981

By C. Feng, W. E. Krul

A study was made of the development of texture and the anisotropy in plastic flow of Ti-8Al-1Mo-1V alloy. Based on Pole figure determinations, the shifting of texture induced by rolling at approximately 400°C was found to be due primarily to slip rotation for the major Portion of the material. Grain boundary shear is believed to be an important factor. The anisotropy of the textured alloy was examined in terms of the variations of yield stress under tension and the ratio of bi -axial strain increments µp, in the temperature range 25" to 290°C. The results were related to Hill&apos;s theory on plastic anisotropy. The Schmid factors of (1100)[1120], (1101)[1120/, and (1101)[1120] slip systems were analyzed and found to be compatible with the observed anisotropy. Cross-slip between these planes was proposed as a possible deformation mode. In a number of published articles, considerable interest has been directed to the possible achievement of texture hardening in hcp metals. Following Backofen, Hosford, and Burke,&apos; this phenomenon was related to the yield criteria of the material and was expressed in terms of the biaxial strain ratio, r = d?w/d?l. The higher the value of r, the greater is the expected potential for texture hardening under certain loading conditions. For a given material, r varies with direction. Such variation can be traced to the anisotropy in plastic flow and can be explained within the framework of the various modes of deformation. Hatch2 found that a high r value coincides with a texture whereby the (0001) pole is closely aligned with the surface normal for sheet materials, Based on the analysis of the slip on the {1010}, {1011}, and (0001) planes, Lee and Backofen3 and Avery, Hosford, and Backofen4 concluded that the resistance to thinning is reduced by the operation of the (0001) <1120> slip system; with this reasoning they were able to explain the low r values (i.e., r « 1) observed in magnesium alloy sheets in the rolling direction and in commercially pure titanium in the transverse direction. The general equation, dealing with plastic flow in a polycrystalline aggregate has been used to correlate the plastic anisotropy and texture. In this expression, T and s are shear and normal stresses, and dri and d? are shear and normal strain increments, respectively. Assuming that five slip systems are operative within each grain and applying the principle of maximum work,5,6 one can determine the m value among the available systems. On this basis, Hosford7 and Chin, Nesbitt, and Williams&apos; were able to correlate m with yield stress under plane-strain compression, and Svensson9 was able to predict the variation of yield stress in textured aluminum. These workers made their analyses from materials in which slip operation is known to be associated with plastic flow. Questions remain regarding the derivation of Hill&apos;s theory on plastic anisotropy,10,11 since it was formulated on von Mises&apos; yield criterion.&apos;&apos; Its ability to deal with other forms of deformation has been in doubt.13 Others have discussed the validity of Hill&apos;s quadratic equation relating strain and yield stress.14&apos;15 For hcp titanium, deformation by various modes of slip and twinning operations has been reported.16-20 If all possible modes of deformation operate and contribute substantially to the plastic flow, it is difficult to imagine how the quadratic expression can suitably describe the anisotropic plastic flow of titanium alloys. Backofen and Hosford15 considered that Hill&apos;s is a macroscopic theory and implied that the major mode of deformation by slip mechanism will adequately describe anisotropy of the material. In the present investigation, slip operation will be shown to play the major role in the development of sheet texture induced by rolling of a commercial titanium alloy. Although twinning and other modes of deformation may also operate, their operation is believed to be secondary. The anisotropic properties of the sheet, which can be expressed in terms of directional variation of r, µp = -d?w/d?l and the yield stress will be shown to be governed primarily by slip operation. MATERIALS AND EXPERIMENTAL TECHNIQUES The titanium alloy chosen for the present investigation had a nominal composition of 8 wt pct Al, 1 wt pct Mo, 1 wt pct V, and 0.1 wt pct interstitial impurities. Sheets varying between 0.1 and 0.15 in. thickness were used. The alloy was received in a condition which was prepared by rolling at 900°C and annealing at 700°C. Subsequently, the sheets were subjected to further reduction in thickness by rolling at 400°C. A total reduction in thickness of 65 to 70 pct was obtained by a series of quick passes in a rolling mill with intermediate reheating. Further reduction in thickness was not possible due to cracking developed at the edges of the sheets. X-ray measurements were conducted in a Siemens and a Norelco unit to determine the texture of the sheets. Reflection techniques were used exclusively with CuK, radiation and a nickel filter. The loss of X-ray intensity due to geometric defocusing was calibrated with a technique described previously." The (0001), (1010), and (1071) pole figures were plotted from 0 to 80 deg, and to present the texture elements quantitatively, inverse pole figures were constructed following the technique described by Jetter, McHargue, and Williams.22 Tensile experiments were carried out at 25", 175",

Jan 1, 1970

By R. T. DeHoff

In any structural transfortnation which is driven by surface tension, the geometric variable of fimdamental importance is the local value of the mean surface curvatuve. Acting through the suvface free energy, this quantity determines the magtnitude of both the pressure and the chemical potential that develops in the neighborhood of an arbitrarily curved surface. A metallographic method which would permit the quaniitatiue estinzation of this propevty is of fundarnerztal irztevest to studies of such processes. In the present paper, it is shoun that the average value of the mean surface curvature in a structuve can be estimated from two simple counting measuretnents made upon a vepresentative metallograpIzic section. No simplifyirlg geonzetric assurmptions are necessary to this deviuation. It is further shoum that the result may be applied to parts of interfaces, e.g., interparticle welds in sintering, or the edge of growing platelets in a phase transformation, without loss of validity. In virtually every metallurgical process in which an interface is important, the local value of the mean surface curvature is the key structural property. This is true because the mean curvature determines the chemical potential of material adjacent to the surface, as well as the state of stress of that material. The theoretical description of such broadly different processes as sintering,1,2 grain growth,3 particle redistrib~tion4,5 and growth of Widmanstatten platelets8 all have as a central geometric variable the "local value of the mean surface curvature". The tools of quantitative metallography currently available permit the statistically precise estimation of the total or extensive geometric properties of a structure: the volume fraction of any distinguishable part:-&apos; the total extent of any observable interface,10,11 and the total length of some three-dimensional lineal feature:&apos; and, if some simplifying assumptions about particle shape are allowed, the total number of particles.&apos;2"3 The size of particles in a structure, specified by a distribution or a mean value, can only be estimated if the particles are all the same shape, and if this shape is relatively simple.14-16 The relationships involved in converting measurements made upon a metallographic section to properties of the three dimensional structure of which the section is a sample are now well-established, and their utility amply demonstrated. In the present paper, another fundamental relationship is added to the tools of quantitative metallography. This relationship is fundamental in the sense that its validity depends only upon the observation of an appropriately representative sample of the structure, and not upon the geometric nature of the structure itself. It involves a new sampling procedure, devised by Rhines, called the "area tangent count". It will first be shown that the "area tangent count" is simply related to the average value of the curvature of particle outline in the two-dimensional section upon which the count is performed. The average curvature of such a section will then be shown to be proportional to the average value of the Mean surface curVature of the structure of which the section is a sample. The final result of the development is thus a relationship which permits the evaluation of the average value of the mean surface curvature from relatively simple counting measurements made upon a representative metallographic section. The result is quite independent of the geometric or even topological nature of the interface being studied. QUANTITATNE EVALUATION OF AVERAGE CURVATURE IN TWO DIMENSIONS The Area Tangent Count. Consider a two-dimen-sional structure composed of two different kinds of distinguishable areas (phases), Fig. l(a). If the system is composed of more than two "phases", it is possible to focus attention upon one phase, and consider the remaining structure as the other phase. The reference phase is separated from the rest of the structure by a set of linear boundaries, of arbitrary shapes and sizes. These boundaries may be totally smooth and continuous, or piecewise smooth and continuous. An element of such a boundary, dA, is shown in Fig. l(b). One may define the "angle subtended" by this arbitrarily curved element of arc, dO, as the angle between the normals erected at its ends, Fig. l(c). Now consider the following experiment. Let a line be swept across this two-dimensional structure, and let the number of tangents that this line forms with elements of arc in the structure be counted. This procedure constitutes the Rhines Area Tangent Count. Suppose that this experiment were repeated a large number of times, with the direction of traverse of the sweeping lines distributed uniformly over the semicircle of orientation.&apos; Those test lines which ap- proach from orientations which lie in the range O to O + dO form a tangent with dA; those outside this range do not, see Fig. l(c). Since the lines are presumed to be uniformly distributed in direction of traverse, the fraction of test lines which form a tangent with dA is the fraction of the circumference of a semicircle which is contained in the orientation range, dO; i.e., vdO/nr or dB/n. If the number of test lines is N, the number forming tangents with dA is N(d0/n). Since each test line sweeps the entire area of the sample, the total area traversed by all N test lines is NL2. The number of tangents formed with dA, per unit area of structure sampled, is therefore

Jan 1, 1968

By D. S. Gleason, D. E. Severson, D. R. Skidmore

Pittsburg and Midway Coal Co. has modified the German Pott-Broche process, on which patents date back to 1927, to produce on a bench scale liquid products by solution hydrogenation of coal. A continuing program of lignite solution-hydro gena-tion experiments is directed toward investigating coal solution reactions, determining favorable conditions for the solution refining of lignite by the Pott-Broche process, and investigating some of the uses for the de-ashed product obtained from lignite The German Pott-Broche process1" on which patents date back to 1927, has been modified by the Pittsburg and Midway Coal Co., a Gulf Oil subsidiary, to produce on a bench scale liquid products by solution -hydrogena-tion of coal." The objectives of the present effort are to investigate coal solution reactions, to determine favorable conditions for the solution refining of lignite by the Pott-Broche process, and to investigate some of the uses for the de-ashed product obtained from lignite. This paper is a summary of results to date in a continuing program of lignite solution-hydrogenation experiments. The coal solution reaction program has several principal aims. The first of these is to determine whether lignite can be successfully dissolved in solvents that might be practical for commercial development. The second object is to determine whether the solvents function after successive cycles of use, recovery, and reuse. It seems necessary to the economics of a potential commercial process that the solvent be recycled. Third, it is desired to learn something about the distribution of the ash constituents between cake and filtrate. The extent of ash removal is important. The nature and quantity of mineral matter passing through the filter may determine end-use marketability. For certain use applications, trace quantities of certain minerals can be objectionable, e.g., titanium and vanadium must be very low in electrode carbon for aluminum production. The Solution Reaction The coal solution Process involves an extremely complex system of chemical reactions. An initial solvent such as anthracene oil is a mixture of hundreds of different compounds with a boiling range of roughly 500" to 750°F at atmospheric pressure. The coal macro-molecule is broken down by thermal decomposition and solvent action into myriads of different compounds, some the same as those comprising the solvent. This similarity in structures opens up the possibility of production and subsequent recovery of solvent. Some solvent is inevitably lost by reaction. Regeneration of solvent was not a problem in the early German Pott-Broche plant. The coal refinery was an integral part of a petroleum refinery complex and replacement solvent was readily available. A coal refinery using lignite, however, might be isolated from other hydrocarbon processing facilities and the regenerability of solvent could be vital to the economic success of the venture. Several structural features of the solvent molecules have been cited as important to the coal solution process.&apos;. The first of these is aromaticity of the material, the second, ability to transfer hydrogen to another molecule, as for example the ability of tetralin to transfer hydrogen and be converted to naphthalene. Finally, the presence of hydroxyl groups on aromatic rings within the molecule, i.e., phenolic character, seems beneficial. Mixtures of pure compounds have been tried by various investigators. Mixtures of o-cresol, a phenolic substance, and tetralin were found to dissolve bituminous coal better than either substance alone.3 This maximum solubility was not found with lignite." Hydrogen contributes to the reaction by hydro-genolysis and by combining with free radicals and molecular "loose ends" to stabilize the compounds formed in coal depolymerization. High boiling point, and correspondingly high molecular weight, seems to be a property which improves solution potential for coal with a given type of compound.&apos; The maceral components of the coal appear to have an important bearing on its ease of solution. The fusain portion is quite inert to solvent action, but the an-thraxylon material dissolves quite readily.3 The hydrogenation reaction can be improved by the use of a catalyst; commercial hydrogenation catalysts having been found effective. Although cost is involved in the use of catalyst and catalyst recovery, the resulting saving in time and perhaps lowered temperature or pressure might justify their use in the solution refining process and decrease the total process costs. Apparatus and Procedure The coal solution runs were made in a 1-gal stainless steel stirred autoclave. The autoclave was provided with thermocouple wells and a transducer to permit continuous recording of temperature and pressure. The autoclave stirrer was magnetically driven, eliminating the leakage inherent with a rotating pressure seal. For runs in which a catalyst was used, the catalyst in the form of beads was placed in a wire mesh container mounted on the stirrer shaft. A control system programmed the heatup and reaction cycle. The permissible heating rate was 5°F per min because of the need to minimize thermal stress in the autoclave body. The temperature was raised at that rate until the reaction temperature was attained and then the temperature was held constant for the desired length of time. The maximum temperature seldom exceeded the average run temperature by more than 15°F.

Jan 1, 1971

By Donald Warren, J. F. Libsch

HIS investigation originated as a result of a pre-vious experimental study&apos; of the magnetic properties of Fe-Co alloys fabricated by the powder metallurgy technique. Densities of powder compacts prepared for the magnetics investigation varied from 7.45 to 7.70 g per cu cm or from 93 to 95 pct of the experimental value of 8.08 g per cu cm for a fused alloy of the same composition.&apos; While this range of density is considered sufficiently high for most applications, the highest possible density is to be desired for maximum magnetic properties. By applying a technique similar to the one described above to a pure electrolytic iron powder, Rostoker³ was able to achieve a density of 7.895 g per cu cm, which is the highest density ever reported for sintered iron. While Rostoker&apos;s work involved the sintering of an elemental powder rather than a mixture, it was believed that higher densities should also have been obtained for alloys using the above technique because of the recoining operation and the high sintering temperature. Consequently, it was decided to investigate the various factors affecting the density of this alloy with the idea that such a study might lead to higher densities and, as a result, powder alloys having magnetic properties identical with those of the fused alloys. It was believed that the principal reason that near-theoretical densities for the powdered alloy were not obtained was the interference of gases with the normal sintering mechanism. When present during the sintering operation, gases can exert several harmful effects: they can remain on the particle surface and interfere with surface diffusion and plastic flow; they can be released and, under certain conditions, expand the void spaces through gas pressure; or they can remain trapped in the pores and exert a hydrostatic pressure that retards elimination of the pores. Jones,4 Rhines,5 Goetzel," and others have given the effect of gases in the sintering of powder compacts an extensive treatment. Among the more important sources of gases in the sintering process are dissolved gases, adsorbed gases, air entrapped during pressing, and gaseous products of chemical reactions. During sintering adsorbed gases are partly released at a relatively low temperature, while those gases entrapped during pressing cannot escape until their pressure is increased sufficiently through increasing temperature to expand the interpartjcle openings. The remaining adsorbed gases, gaseous reduction products, and dissolved gases produce a similar effect at the higher temperatures. If, in the sintering process, gas evolution occurs after the interpore channels have been sealed, an exaggerated expansion of the void spaces results. This is particularly true if the temperature is high enough for extensive plastic flow. In his fabrication of powder bars from tantalum, Balke7 had to consider the effect of adsorbed hydrogen and provide for its escape during sintering by limiting the compacting pressure to a maximum of 50 tons per sq in. The effect of gases entrapped during pressing was first noted by Trzebiatowski8 when he found that gold and silver powders decrease in density with increasing sintering temperature if pressed at 200 tsi, while they exhibit the usual increase when pressed at 40 tsi. Recent investigators9-11 have also noted that entrapped gases have an effect on the expansion of copper compacts during sintering. Proper provision for the escape of gaseous products of reduction must be made in order to avoid deleterious effects. Myers" states that in the sintering of electrolytic tantalum powder, the temperature was gradually raised to 2600°F with a pause at 2000°F to permit reduction of the oxides. Experimental Details For the present study, 50 pct Co-50 pct Fe compacts in the form of circular disks 1½ in. in diam and 0.15 in. thick were fabricated by the pressing and sintering of a mixture of the elemental powders. It was decided to follow the sintering process by means of liquid permeability measurements, because it was thought that such measurements might serve as a measure of relative pore sizes, as well as a possible indication of the point at which most of the interpore channels become sealed. However, since the permeability as measured by the flow of a liquid, such as ethylene glycol, does not give an absolute indication of the point where the pores have become isolated, a method for determining the percentage of pores connected to the surface was set up. As an additional cross check on the permeability measurements, metallographic methods were used to study the relative pore size. Finally, the property of ultimate interest, the density, was measured. Raw Materials: The powders used consisted of an annealed, 99.9 pct pure, —150 mesh grade of electrolytic iron powder, and a 98 pct pure, —200 mesh grade of reduced and comminuted cobalt powder. The cobalt powder was not further processed either by hydrogen reduction or annealing. The screen analyses for the iron and cobalt powders are given in Table I, while the chemical analyses for each type of powder are listed in Table 11. Table 111 gives the hydrogen loss measurements for the powders according to the M.P.A. Standard Method and for a higher temperature as well. Preparation of Compacts: Equal amounts of the elemental powders were mixed by rotation for 1 hr and then pressed into compacts approximately 0.15

Jan 1, 1952

By R. Silverman, H. Blumenthal

It was found that despite the similarity of chemical analyses of different titanium carbides used as base materials for cermets, the physical properties, especially transverse-rupture strengths, of test bars were different. Hence this metallographic study attempts to link physical properties to micro-structures. It is shown that microstructure, grain shape, and grain growth are functions of three interrelated factors: 1—powder production procedure, 2—surface conditioning of the particles, and 3—impurities either contained in the original powder or acquired during ball milling. An explanation is offered for the "coring effect," long observed, but heretofore of unknown origin. The explanation is based on assumption of an oxide film and on chemical analyses which substantiate these findings. TITANIUM carbide has become in recent years a material of great interest in the high temperature field. Consequently, many manufacturers in the United States and Europe are producing titanium carbide for cermet applications as well as for additions to the well known tungsten carbide tools. All present commercial processes of titanium carbide production utilize the chemical reaction of titanium dioxide and carbon to form as nearly as possible stoichiometric Tic. This reaction is carried out in three ways: 1—in a menstruum of molten metal,&apos; 2—in the solid state, either in a protective atmosphere2 or in vacuum;" or 3—in an are-melting operation. In spite of the fact that the pure carbides obtained in these operations are almost identical chemically, the physical properties vary considerably when they are combined with a binder (Ni, Co) to form cermets. This fact led the authors to examine metal-lographically nickel-bonded titanium carbide in order to find the possible reasons for this behavior. Materials and Methods Five different titanium carbides were used in this investigation. They are identified in Table I. The first four materials were used in the as-received condition. Material E, received in lumps, was crushed to —100 mesh and carried through a flotation process in order to bring its graphite content in line with the other products. A Galagher flotation cell was used with pine oil as frothing agent. The chemical analyses of the investigated materials are given in Table 11. The binder used was carbonyl nickel of 9 to 14 microns particle size, supplied by A. D. Mackay. The materials were ball milled at a ball to charge ratio of 6:1 using procedures described under "Experiments and Results." All particle sizes mentioned are averages determined with a Fisher Sub-sieve Sizer. Test bars (lx0.40x0.16 in.) were prepared by 1—hot pressing to 85 to 95 pct of theoretical density at pressures between 1 and 1½ tsi and temperatures from 1600" to 1800°C, 2-—-cold presssing after 3 pct camphor had been added, or 3—wet pressing, both 2 and 3 at pressures between 5 and 10 tsi. All pressed bars were sintered in a vacuum of 105 to 10-6 mm Hg for 2 hr at 1350 °C. Transverse-rupture strengths were determined by breaking on a Baldwin Universal Testing Machine over a 9/16 in. span. Densities were measured by water displacement. The preparation of the specimens for micrographs was done according to Silverman and Doshna Luscz." All magnifications are at X1000. A sodium picrate electrolytic etch was used. Experiments and Results The influence of ball-milling procedure, ball-milling medium, pressing procedure, and sintering procedure on the microstructure of 80/20 — TiC/Ni were investigated. Ball Milling of Materials A, B, and C in a Steel Mill: Figs. 1 and 2 show microstructures of hot-pressed and vacuum-sintered test bars of materials A and B after the respective materials had been ball milled to 2.1 microns particle size in a steel mill and mixed with 20 pct Ni binder. Material A (Fig. 1) shows considerable grain growth. Also evident is a tendency of the carbide grains to coalesce. The density is 98 pct and the low transverse-rupture strength of 111,000 psi is probably caused by many large grains and an unfavorable packing factor. Almost all grains show a slight indication of "coring." Material B (Fig. 2), although showing grain growth, still has many small particles and a better distribution of binder and carbide due to the relative absence of the coalescing tendency. "Coring" can be observed in almost all grains. The high transverse-rupture strength of 179,000 psi and the density of 100 pct are believed to be due to the many small grains completely surrounded by the binder phase. There is also a preference to form spherical grains with material A, while most grains of material B preserve their angular shapes. Material C, of which no picture is given, stays between A and B in every respect. Rounding of some grains can be observed as well as coring, but the latter to a lesser degree than with material B. Its densification is good and the transverse-rupture strength obtained is 142,000 psi. Ball Milling of Materials A, B, C, and E in a WC Mill: When the Tic powders were ball milled to 2 microns particle size in a we mill, then ball-mill mixed with 20 pct Ni binder, hot pressed, and vacuum

Jan 1, 1956

By J. R. Szedon, T. L. Chu, G. A. Gruber

Amorphous adherent filnzs of silicon dioxide have been deposited on silicon substrates by the oxidation of silane at temperatures ranging from 650 to 1050C. Various diluents (argon, nitrogen, hydrogen) were used to suppress the formation of SiO2 in the gas phase. Deposition rates of the oxide were determined over the temperature range in question as functions of&apos; re-actant flow rates. Etch rate studies were used for a cursory comparison of structural properties of deposited and thermally grown oxides. From electrical evaluation of metal-insulator-silicon capacitors it was determined that the interface charge density of deposited films is similar go that of dry-oxygen-grown films in the 850° to 1050 C temperature range. Deposited films exhibit several ionic instability effects which differ in detail from those reported for thermal oxides. Stable passivating films of silicon nitride over deposited oxides appear to be practical for use in silicon planar device fabrication. Such films can be prepared under temperature conditions which have less effect on substrate impurity distributions than in the case of grown oxides. AMORPHOUS silicon dioxide (silica) is compatible with silicon in electrical properties and is the most widely used dielectric in silicon devices at present. Silica films can be prepared by the oxidation of silicon or deposited on silicon or other substrate surfaces by chemical reactions or vacuum techniques. The ability of thermally grown silicon dioxide films to passivate silicon surfaces forms one of the practical bases of the planar device technology. Properly produced and treated films of grown SiO 2 can have low densities of interface charge (-1 X 10" charges per sq cm) and can be stable as regards fast migrating ionic sgecies. 1 To maintain these properties, even with an otherwise hermetically sealed ambient, the Sia layers must be at least l000 A thick. Such thicknesses require oxidation in dry oxygen for periods of 7.8 hr at 900°C or 2 hr at 1000°C. Although oxidation in steam or wet oxygen can reduce these times to 17 and 5 min, the resulting oxides must be annealed to produce acceptable levels of interface charge., Oxidation or annealing involving moderate to high temperatures for extended periods of time can be undesirable. Under some conditions, there can be changes in the distribution of impurities within the underlying substrate. A chemical deposition technique using gaseous am-bients is particularly attractive and flexible for preparing oxide films. With a wide range of deposition rates available, films can be produced under condi- tions of time and temperature less detrimental to impurity distributions in the silicon than in the case of thermal oxidation. The pyrolysis of alkoxysilanes, the hydrolysis of silicon halides, and various modifications of these reactions are most commonly used for the deposition of silica films.3 Silica films obtained in this manner are likely to be contaminated by the by-products of the reaction, organic impurities, or hydrogen halides. The use of the oxidation of silane for the deposition process has been reported recently.4 The deposition of silica films on single-crystal silicon substrates by the oxidation of silane in a gas flow system has been studied in this work. The deposition variables studied were the crystallographic orientation of the substrate surface, the substrate temperature, and the nature of the diluent gas. The electrical charge behavior of Si-SiO2-A1 structures prepared under various conditions was investigated by capacitance-voltage (C-V) measurements of metal-insulator-semiconductor (MIS) capacitors. The experimental approaches and results are discussed in this paper. 1) DEPOSITION OF SILICA FILMS The overall reaction for the oxidation of silane is: The equilibrium constants of this reaction in the temperature range 500° to 1500°K, calculated from the JANAF thermochemical data,= are shown in Fig. 1. In addition to the large equilibrium constants, the oxidation of silane is also kinetically feasible at room temperature and above. However, the strong reactivity of silane toward oxygen tends to promote the nucleation of silica in the gas phase through homogeneous reactions, and the deposition of this silica on the substrate would yield nonadherent material. The formation of silica in the gas phase can be reduced by using low partial pressures of the reactants. Argon, hydrogen, and nitrogen were used as diluents in this work. 1.1) Experimental. The deposition of silica films by the oxidation of silane was carried out in a gas flow system using an apparatus shown schematically in Fig. 2. Appropriate flow meters and valves were used to control the flow of various reactants, i.e., argon, hydrogen, nitrogen, oxygen, and silane. Semiconductor-grade silane, argon of 99.999 pct minimum purity, oxygen of 99.95 pct minimum purity, and nitrogen of 99.997 pct minimum purity, all purchased from the Matheson Co., were used without further purification. In several instances, a silicon nitride film was deposited over the silica film. This was achieved by the nitridation of silane with ammonia using anhydrous ammonia of better than 99.99 pct purity supplied by the Matheson CO.&apos; The reactant mixture of the desired composition was passed through a Millipore filter into a horizontal water-cooled fused silica tube of 55 mm

Jan 1, 1969